CN110436959A - A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics - Google Patents

A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics Download PDF

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CN110436959A
CN110436959A CN201910699248.4A CN201910699248A CN110436959A CN 110436959 A CN110436959 A CN 110436959A CN 201910699248 A CN201910699248 A CN 201910699248A CN 110436959 A CN110436959 A CN 110436959A
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porous ceramics
hollow ball
alumina
magnesium
aluminate spinel
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罗旭东
侯庆冬
杨孟孟
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University of Science and Technology Liaoning USTL
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract

The invention patent relates to a kind of preparation methods of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, magnesite is crushed to partial size less than 0.074mm first, 30 minutes are kept the temperature through 700-1000 DEG C, activity light-burning magnesium powder is made, using it with alumina hollow ball and alumina powder light-burning magnesium powder as raw material, using aluminum fluoride and magnesium powder is fluorinated as catalyst, starch is as bonding agent and pore creating material, through premix, mixing, molding, drying, firing, obtain with magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics.It is burnt at a lower temperature, and forms magnesium aluminate spinel whisker network skeleton between hollow sphere, further enhance the bending strength of alumina porous ceramic, to obtain high-intensitive, high porosity alumina porous ceramic.

Description

A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics
Technical field
The present invention relates to technical field of inorganic chemical industry, and in particular to a kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball The preparation method of porous ceramics.
Background technique
With the development of modern science and technology section, the especially development in the fields such as metallurgy, chemical industry, auto industry, environmental protection and energy, Requirement to material is more and more harsher, and there is an urgent need to develop a kind of novel high performance structures materials.Energy growing tension, environmental protection Increasingly stringent, thermal insulation material is low to the performance such as thermal conductivity of some keys as the indispensable a part of hot industry, resistance to Fiery degree is high, and applied at elevated temperature volume stability is good, and thermal shock resistance is good etc. has also been proposed new requirement, to meet light structures high temperature The demand of kiln.The light weeight alumina brick prepared on domestic market by burning mistake method or foaming, lightweight magnesium-aluminum spinel brick, gently Matter clay brick, light silicious brick etc. have been widely used for the back sheet and thermal insulation layer of Industrial Stoves.But be applied to high temperature or The work face brick of person's superhigh temperature Industrial Stoves is mainly alumina bubble brick.Usual alumina hollow ball insulation product is to aoxidize Aluminium hollow sphere adds appropriate bonding agent using alpha-alumina as matrix for aggregate, is prepared through molding, drying and firing;It is high Matrix is in densifie state after temperature sintering, leads to the big (1.4-1.6g/cm of conventional aluminium oxide hollow sphere insulating product density3), thermal conductivity Rate is high, and accumulation of heat is big, and it is excessively high to ultimately cause hot industry energy consumption, energy-saving unfavorable in reducing kiln weight.And due to using Conventional sintering neck combined aluminum oxide hollow sphere, causes the intensity of sample lower.The present invention aiming at the shortcomings of the prior art, provides A kind of preparation method of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics.
Summary of the invention
The present invention provides a kind of preparation methods of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, with oxygen Change aluminium hollow sphere, alumina powder and light-burning magnesium powder are raw material, and using aluminum fluoride and fluorination magnesium powder as catalyst, starch is as knot Mixture and pore creating material obtain hollow with magnesium aluminate spinel whisker reinforcement aluminium oxide through premix, mixing, molding, drying, firing Ball porous ceramics.It is burnt at a lower temperature, and forms magnesium aluminate spinel whisker network skeleton between hollow sphere, further The bending strength of alumina porous ceramic is enhanced, to obtain high-intensitive, high porosity alumina porous ceramic.
To achieve the above object, the invention is realized by the following technical scheme:
A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, which is characterized in that with alumina hollow ball be make Hole agent, using alumina powder and light-burning magnesium powder as high-temperature agglomerant, aluminum fluoride and magnesium fluoride are as catalyst, and starch is as bonding agent And pore creating material obtains the alumina hollow ball with magnesium aluminate spinel whisker reinforcement through premix, mixing, molding, drying, firing Porous ceramics, specific steps are as follows:
Magnesite is crushed to partial size less than 0.074mm, keeps the temperature 30 minutes through 700-1000 DEG C, it is light-burned that activity is made by step 1 Magnesium powder;In parts by weight, alumina hollow ball, 18-25 parts of partial size that 65-70 parts of partial size is 3-0.074mm are less than The light-burning magnesium powder of alumina powder, 8-10 parts of partial size less than 0.074mm, 1-4 parts of the partial size of 0.074mm is less than 0.074mm's Aluminum fluoride and 1-4 parts of partial size are less than the magnesium fluoride of 0.074mm, are sufficiently premixed in blender, obtain premix material;
Step 2 is subject to the water of pre-composition material weight 5-8% and the starch of 5-10% into the premix material of step 1 outside, is placed in mixed Continue to be kneaded 10-20 minutes in mill, the pug after being kneaded;
Pug after mixing is put into mold and carries out molding casting by step 3, after sample conserves 24-48 hours in a mold Demoulding forms porous ceramics green body;
Step 4, it is dry, the porous ceramics green body after demoulding is 24-48 hours dry under conditions of 110 DEG C;
Porous ceramics green body after drying is warming up in high temperature furnace 1350-1550 DEG C, calcined 2-6 hours, then drop by step 5 Temperature keeps the temperature 2-6 hours to 650-850 DEG C, finally with taking-up after furnace natural cooling to get to magnesium aluminate spinel whisker reinforcement Alumina hollow ball porous ceramics.
Preferred calcination time is 2-4 hours in the step 5.
Compared with prior art, the beneficial effects of the present invention are: 1) magnesium aluminate spinel whisker reinforcement prepared by the present invention Alumina hollow ball ceramics, by resourceful Al2O3, MgO matter raw material preparation, it is low in cost;2) magnesium aluminate spinel whisker has Excellent high temperature resistant, corrosion-resistant, superior thermal shock resistance and mechanical property, being introduced into porous ceramic film material can be improved material Toughness, increase impact strength, be conducive to improve ceramic material service life.3) whisker can play the work of toughening to brick body With the excessive toughening effect of the draw ratio of whisker is poor, and draw ratio is too small, and product can't be whisker, referred to as crystal grain, major diameter Than for reinforcing effect between 10 ~ 70 it is best.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Preparation method of the invention is described further below with reference to embodiment:
Embodiment 1:
A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, which is characterized in that with alumina hollow ball be make Hole agent, using alumina powder and light-burning magnesium powder as high-temperature agglomerant, aluminum fluoride and magnesium fluoride are as catalyst, and starch is as bonding agent And pore creating material obtains the alumina hollow ball with magnesium aluminate spinel whisker reinforcement through premix, mixing, molding, drying, firing Porous ceramics, specific steps are as follows:
Magnesite is crushed to partial size less than 0.074mm, keeps the temperature 30 minutes through 700 DEG C, activity light-burning magnesium powder is made by step 1; 70kg partial size is small less than alumina powder, the 8.4kg partial size of 0.074mm for alumina hollow ball, the 18kg partial size of 3-0.074mm It is less than the fluorination of 0.074mm in aluminum fluoride of the light-burning magnesium powder, 1.8kg partial size of 0.074mm less than 0.074mm and 1.8kg partial size Magnesium is sufficiently premixed in blender, obtains premix material;
Step 2 is subject to 6kg water and 5kg starch into the premix material of step 1 outside, is placed in kneading machine and continues to be kneaded 20 points Clock, the pug after being kneaded;
Pug after mixing is put into mold and carries out molding casting by step 3, takes off after sample conserves 24 hours in a mold Mould forms porous ceramics green body;
Step 4, the porous ceramics green body after demoulding is 25 hours dry under conditions of 110 DEG C;
Porous ceramics green body after drying is warming up in high temperature furnace 1350 DEG C, calcined 2 hours, then be cooled to 650 by step 5 DEG C, 2 hours are kept the temperature, finally with taking-up after furnace natural cooling to get to magnesium aluminate spinel whisker reinforcement alumina hollow ball Porous ceramics.
The draw ratio of magnesium aluminate spinel whisker in porous ceramics manufactured in the present embodiment is 21.2, and strength at normal temperature is 7.3MPa, apparent porosity 75.5%.
Embodiment 2:
A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, which is characterized in that with alumina hollow ball be make Hole agent, using alumina powder and light-burning magnesium powder as high-temperature agglomerant, aluminum fluoride and magnesium fluoride are as catalyst, and starch is as bonding agent And pore creating material obtains the alumina hollow ball with magnesium aluminate spinel whisker reinforcement through premix, mixing, molding, drying, firing Porous ceramics, specific steps are as follows:
Magnesite is crushed to partial size less than 0.074mm, keeps the temperature 30 minutes through 800 DEG C, activity light-burning magnesium powder is made by step 1; Alumina powder, the 9kg partial size of alumina hollow ball, 19kg partial size less than 0.074mm that 68kg partial size is 3-0.074mm are less than The aluminum fluoride of light-burning magnesium powder, 2kg partial size less than 0.074mm and 2kg partial size of 0.074mm are less than the magnesium fluoride of 0.074mm, are stirring It mixes in machine and is sufficiently premixed, obtain premix material;
Step 2 is subject to 7kg water and 6kg starch into the premix material of step 1 outside, is placed in kneading machine and continues to be kneaded 15 points Clock, the pug after being kneaded;
Pug after mixing is put into mold and carries out molding casting by step 3, takes off after sample conserves 24 hours in a mold Mould forms porous ceramics green body;
Step 4, the porous ceramics green body after demoulding is 30 hours dry under conditions of 110 DEG C;
Porous ceramics green body after drying is warming up in high temperature furnace 1450 DEG C, calcined 3 hours, then be cooled to 650 by step 5 DEG C, 2 hours are kept the temperature, finally with taking-up after furnace natural cooling to get to magnesium aluminate spinel whisker reinforcement alumina hollow ball Porous ceramics.
The draw ratio of magnesium aluminate spinel whisker in porous ceramics manufactured in the present embodiment is 61.2, and strength at normal temperature is 13.7MPa, apparent porosity 67.5%.
Embodiment 3:
A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, which is characterized in that with alumina hollow ball be make Hole agent, using alumina powder and light-burning magnesium powder as high-temperature agglomerant, aluminum fluoride and magnesium fluoride are as catalyst, and starch is as bonding agent And pore creating material obtains the alumina hollow ball with magnesium aluminate spinel whisker reinforcement through premix, mixing, molding, drying, firing Porous ceramics, specific steps are as follows:
Magnesite is crushed to partial size less than 0.074mm, keeps the temperature 30 minutes through 900 DEG C, activity light-burning magnesium powder is made by step 1; 65kg partial size is small less than alumina powder, the 9.2kg partial size of 0.074mm for alumina hollow ball, the 21kg partial size of 3-0.074mm It is less than the fluorination of 0.074mm in aluminum fluoride of the light-burning magnesium powder, 2.4kg partial size of 0.074mm less than 0.074mm and 2.4kg partial size Magnesium is sufficiently premixed in blender, obtains premix material;
Step 2 is subject to 8kg water and 7kg starch into the premix material of step 1 outside, is placed in kneading machine and continues to be kneaded 10 points Clock, the pug after being kneaded;
Pug after mixing is put into mold and carries out molding casting by step 3, takes off after sample conserves 36 hours in a mold Mould forms porous ceramics green body;
Step 4, the porous ceramics green body after demoulding is 35 hours dry under conditions of 110 DEG C;
Porous ceramics green body after drying is warming up in high temperature furnace 1550 DEG C, calcined 3 hours, then be cooled to 650 by step 5 DEG C, 2 hours are kept the temperature, finally with taking-up after furnace natural cooling to get to magnesium aluminate spinel whisker reinforcement alumina hollow ball Porous ceramics.
The draw ratio of the magnesium aluminate spinel whisker of alumina hollow ball porous ceramics manufactured in the present embodiment is 10.1, room temperature Flexural strength is 9.5MPa, apparent porosity 60.1%.

Claims (2)

1. a kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics, which is characterized in that be with alumina hollow ball Pore creating material, using alumina powder and light-burning magnesium powder as high-temperature agglomerant, aluminum fluoride and magnesium fluoride are as catalyst, and starch is as combination Agent and pore creating material obtain having the aluminium oxide of magnesium aluminate spinel whisker reinforcement hollow through premix, mixing, molding, drying, firing Ball porous ceramics, specific steps are as follows:
Magnesite is crushed to partial size less than 0.074mm, keeps the temperature 30 minutes through 700-1000 DEG C, it is light-burned that activity is made by step 1 Magnesium powder;In parts by weight, alumina hollow ball, 18-25 parts of partial size that 65-70 parts of partial size is 3-0.074mm are less than The light-burning magnesium powder of alumina powder, 8-10 parts of partial size less than 0.074mm, 1-4 parts of the partial size of 0.074mm is less than 0.074mm's Aluminum fluoride and 1-4 parts of partial size are less than the magnesium fluoride of 0.074mm, are sufficiently premixed in blender, obtain premix material;
Step 2 is subject to the water of pre-composition material weight 5-8% and the starch of 5-10% into the premix material of step 1 outside, is placed in mixed Continue to be kneaded 10-20 minutes in mill, the pug after being kneaded;
Pug after mixing is put into mold and carries out molding casting by step 3, after sample conserves 24-48 hours in a mold Demoulding forms porous ceramics green body;
Step 4, it is dry, the porous ceramics green body after demoulding is 24-48 hours dry under conditions of 110 DEG C;
Porous ceramics green body after drying is warming up in high temperature furnace 1350-1550 DEG C, calcined 2-6 hours, then drop by step 5 Temperature keeps the temperature 2-6 hours to 650-850 DEG C, finally with taking-up after furnace natural cooling to get to magnesium aluminate spinel whisker reinforcement Alumina hollow ball porous ceramics.
2. a kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics according to claim 1, feature exist In preferred calcination time is 2-4 hours in the step 5.
CN201910699248.4A 2019-07-31 2019-07-31 A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics Pending CN110436959A (en)

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CN108947568A (en) * 2018-08-16 2018-12-07 中钢集团洛阳耐火材料研究院有限公司 A method of alumina bubble brick is prepared using pore creating material
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Application publication date: 20191112